CN105788882B - The hydrothermal preparing process of cobaltosic oxide nano cube and the application for preparing electrode slice - Google Patents
The hydrothermal preparing process of cobaltosic oxide nano cube and the application for preparing electrode slice Download PDFInfo
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- CN105788882B CN105788882B CN201610265839.7A CN201610265839A CN105788882B CN 105788882 B CN105788882 B CN 105788882B CN 201610265839 A CN201610265839 A CN 201610265839A CN 105788882 B CN105788882 B CN 105788882B
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Abstract
The present invention relates to the hydrothermal preparing process of cobaltosic oxide nano cube and prepare the application of electrode slice；Cobalt salt, alkali, surfactant is weighed respectively to dissolve in deionized water；It respectively takes isometric cobalt salt solution, aqueous slkali to carry out water bath with thermostatic control respectively, after agitating and heating is uniform, aqueous slkali is added in cobalt salt solution, surfactant solution is added after the reaction was complete, obtains mixed solution；Mixed solution is transferred in sealed shell of tank and carries out hydro-thermal process, obtains black precipitate；Black precipitate is washed through deionized water, absolute ethyl alcohol successively, it is dry under air atmosphere, obtain the cobaltosic oxide nano cube.The cobaltosic oxide nano cube is mixed with conductive agent and binder, slurry is obtained after stirring；The slurry is uniformly scraped into Tu in pretreated nickel foam, dry, tabletting is to get the electrode slice.Appointed condition is simpler needed for preparation method of the present invention, easy to operate, and manufacturing cost is low, is suitable for batch production large-scale production.
Description
Technical field
The present invention relates to a kind of preparation methods of electrode material for super capacitor, and in particular to a kind of cobaltosic oxide nano
Cube hydrothermal preparing process method and prepare the application of electrode slice.
Background technology
The features such as ultracapacitor is because of its high-energy density, long charge and discharge cycles period and high energy source efficiency, it is considered to be
The alternative energy source with high application potential stores option in following electric vehicle and wearable mobile electronic device.
In above application, ultracapacitor can provide necessary high energy acceleration and storage brake energy for electric vehicle, while for that can wear
It wears mobile electronic device and the electric energy needed for continuing a journey for a long time is provided.
In recent years, more and more researchers are also resulted in for the research and development of high-performance super capacitor electrode material
Concern, specifically, electrode material for super capacitor is broadly divided into two major classes：Electric double-layer capacitor based on carbon-based material
Device electrode material, the fake capacitance electrode material based on transition group metallic oxide or conducting polymer.Electric double layer capacitance
Device at work, mainly makes the positive and negative charge in solution gather in anisotropic energization carbon-based material electrode surface, forms thickness and exists
0.5nm charge layers below, to achieve the purpose that store electric energy.It is suitable as the mainly transition group of fake capacitance electrode material
Metal oxide, because these metals have varying chemical valence state, it is anti-redox can to occur in certain voltage range
It answers, energy is stored by converting electrical energy into chemical energy.Theoretically, magnesium-yttrium-transition metal material such as yttrium oxide, ruthenium-oxide, dioxy
Change manganese etc. and be satisfied by basic demand as electrode material for super capacitor, but in practical applications, it is contemplated that yttrium oxide and
Ruthenium-oxide selling at exorbitant prices, manganese dioxide theoretical specific capacity is relatively low, therefore does not have large-scale application foreground.And cobaltosic oxide
Then due to its high theoretical specific capacity value (up to 3500F/g), low cost, Environmental compatibility is good the advantages that become most potential
Fake capacitance electrode material.
For cobaltosic oxide material, existing frequently-used preparation method has two classes：Electrodeposition process, hydro-thermal method.It is well known that
There is the shortcomings of repeatability is poor, product component is impure, influence factor is complicated in application process in electro-deposition method.And hydro-thermal method
It is then simple to operation, it can guarantee higher repeatability.Currently used hydro-thermal method prepares cobaltosic oxide material, generally requires
Cobalt hydroxide is first prepared as presoma, then carries out subsequent calcination oxidation processes to it, either simplex skill is not cumbersome for this preparation method,
Production cost is also improved, and in the high-temperature calcination in later stage, it is easy to which a degree of destruction is caused to the pattern of presoma.
Invention content
It is an object of the invention to overcome above-mentioned the shortcomings of the prior art, a kind of cobaltosic oxide nano cube is provided
Hydrothermal preparation method.Our one step hydro thermal method is relatively easy, and corner angle obtained are clearly demarcated, and the cobaltosic oxide of uniform particle diameter is received
Meter Li Fang has splendid energy storage application prospect.Up to the present, this to prepare cobaltosic oxide with one step hydro thermal method and receive
The method of meter Li Fang there is no relevant report both at home and abroad.
The purpose of the present invention is what is be achieved through the following technical solutions：
The present invention provides a kind of preparation method of cobaltosic oxide nano cube, and described method includes following steps：
1) cobalt salt, alkali, surfactant are weighed respectively to dissolve in deionized water, obtain 40~60g/L cobalt salt solutions, 55
~77g/L aqueous slkalis, 6~10g/L surfactant solutions；
2) isometric cobalt salt solution, aqueous slkali is respectively taken to carry out water bath with thermostatic control respectively, after agitating and heating is uniform, by alkali
Solution is added in cobalt salt solution, and surfactant solution is added after the reaction was complete, obtains mixed solution；
3) mixed solution is transferred in sealed shell of tank, under air-proof condition, contains cobalt salt, alkali, surfactant to described
Mixed solution carry out hydro-thermal process, obtain black precipitate；
4) black precipitate is washed through deionized water, absolute ethyl alcohol successively, it is dry under air atmosphere, obtain described four
Co 3 O nano cubic.
Preferably, in step 1, the cobalt salt be cobalt acetate, cobalt nitrate or cobaltous sulfate, the alkali be sodium hydroxide or
Potassium hydroxide；The surfactant is polyethylene glycol -200, neopelex or lauryl sodium sulfate.
Preferably, in step 2, the temperature setting of the constant temperature water bath is 45~55 DEG C；Added surfactant solution
Volume be cobalt salt solution volume 10~15%；The stirring is carried out using electric mixing device, and the rotating speed of described device is
200~500 revs/min.
Preferably, in step 3, the temperature setting of the hydro-thermal reaction is 130~180 DEG C, and the time of hydro-thermal process is arranged
It is 30~40 hours.
Preferably, in step 4, the temperature setting of drying temperature is 60~90 DEG C in the drying box.
Application of the cobaltosic oxide nano cube in preparing electrode slice made from method using the present invention, by described four
Co 3 O nano cubic is mixed with conductive agent and binder, and slurry is obtained after being sufficiently stirred；By the slurry uniformly scrape Tu in
In pretreated nickel foam, dry, tabletting is to get the electrode slice.
The mass ratio of the cobaltosic oxide nano cube, conductive agent and binder is 8~7.5:1~1.5:1；It is described to lead
Electric agent is porous activated carbon or acetylene black, and the binder is PTFE ethanol solutions.
The drying temperature is 50~80 DEG C, and pressure is 13~15MPa when the tabletting.
The conductive agent is porous activated carbon or acetylene black, and binder is PTFE ethanol solutions；The cobaltosic oxide
The mass ratio of nano cubic, activated carbon and binder is 8:1:1；The cobaltosic oxide nano cube, acetylene black and binder
Mass ratio be 7.5:1.5:1.
Compared with prior art, the present invention has following advantageous effect：
(1) appointed condition needed for preparation method of the present invention is simpler, and easy to operate, manufacturing cost is low, is suitable for batch production
Large-scale production.
(2) present invention prepares cobaltosic oxide nano cube using one step hydro thermal method, is not necessarily to subsequent calcination oxidation process, can
Repeated high, the pattern control of product can be effectively ensured, and preparation process flow is greatly simplified.It is prepared simultaneously
The specific capacitance better performances of cobaltosic oxide nano cube, while there is excellent cyclical stability.
Description of the drawings
Fig. 1 is the transmission electron microscope picture for the cobaltosic oxide nano cube that this method is prepared.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1
Cobaltous sulfate, sodium hydroxide and ethylene glycol -200 are made into deionized water to cobalt sulfate solution, the 55g/ of 40g/L respectively
- 200 solution of sodium hydroxide solution and 6g/L polyethylene glycol of L.Cobalt sulfate solution and sodium hydroxide are respectively taken one liter, are put into simultaneously
It is kept for 5 minutes in 45 DEG C of constant temperature water bath, then sodium hydroxide is added in cobalt sulfate solution, using 200 revs/min of rotating speeds
Uniform stirring, it can be seen that solution colour changes, and reacts and acutely carries out, and after reaction carries out ten minutes, is added 100 milliliters
- 200 solution of ethylene glycol is add to the above mixed solution, and mixed solution is transferred in hydrothermal device and is handled, temperature is set
Be set to 130 DEG C, when it is 40 hours a length of.It waits after the completion of reacting, by gained black precipitate respectively through deionized water, washes of absolute alcohol
Centrifugation 3 times, it is 10 hours dry at 60 DEG C in air drying cabinet, obtain cobaltosic oxide product.
It is 8 in mass ratio by product and acetylene black and PTFE binders:1:1 uniformly mixing, the slurry mixed is applied
It is layed onto above nickel foam, is placed into the air drying cabinet that temperature setting is 50 DEG C and processing is dried.To the electrode handled well
Piece compressing tablet process, pressure are set as 12Mpa, finally carry out electrochemical property test, show that its specific capacitance is 360F/g.
Embodiment 2
The cobalt acetate that cobalt acetate, sodium hydroxide and neopelex are made into deionized water to 50g/L respectively is molten
Liquid, the sodium hydroxide solution of 65g/L and 8g/L neopelex solution.Cobalt acetate solution and sodium hydroxide are respectively taken one
It rises, while being put into 55 DEG C of constant temperature water bath and being added 5 minutes, then sodium hydroxide is added in cobalt acetate solution, use
350 revs/min of rotating speed uniform stirrings, it can be seen that solution colour changes, and reacts and acutely carries out, and waits for that reaction carries out ten minutes
Afterwards, 120 milliliters of neopelex solution are added to be add to the above mixed solution, mixed solution is transferred to hydro-thermal dress
Handled in setting, temperature setting be 160 DEG C, when it is 36 hours a length of.It waits after the completion of reacting, by gained black precipitate respectively through going
Ionized water, washes of absolute alcohol centrifuge 3 times, 8 hours dry at 80 DEG C in air drying cabinet, and it is vertical to obtain cobaltosic oxide nano
Side, nanoparticle size are about 80nm, uniform particle sizes, favorable dispersibility.
It is 7.5 in mass ratio by product and activated carbon and PTFE binders:1.5:1 uniformly mixing, the slurry that will be mixed
Material is coated to above nickel foam, is placed into the air drying cabinet that temperature setting is 65 DEG C and processing is dried.To what is handled well
Electrode slice compressing tablet process, pressure are set as 14Mpa, finally carry out electrochemical property test, show that its specific capacitance is 570F/g.Figure
The transmission electron microscope picture of 1 cobaltosic oxide nano cube being prepared for this method；As shown in Figure 1, it can be prepared with this method
Obtain the cobaltosic oxide nano cube of uniform particle sizes, cube pattern is very regular, and granule-morphology have it is fabulous complete
Property.
Embodiment 3
Cobalt nitrate, potassium hydroxide and lauryl sodium sulfate are made into deionized water respectively 60g/L cobalt nitrate solution,
The potassium hydroxide solution and 10g/L sodium dodecyl sulfate solutions of 77g/L.Cobalt nitrate solution and potassium hydroxide are respectively taken one liter,
It is put into 55 DEG C of constant temperature water bath and is added 5 minutes simultaneously, then potassium hydroxide is added in cobalt nitrate solution, using 500
Rev/min rotating speed uniform stirring, it can be seen that solution colour changes, and reacts and acutely carries out, and after reaction carries out ten minutes, adds
Enter 150 milliliters of sodium dodecyl sulfate solutions to be add to the above mixed solution, by mixed solution be transferred in hydrothermal device into
Row processing, temperature setting be 180 DEG C, when it is 30 hours a length of.It waits after the completion of reacting, by gained black precipitate respectively through deionization
Water, washes of absolute alcohol centrifuge 3 times, 8 hours dry at 90 DEG C in air drying cabinet, obtain cobaltosic oxide product.
It is 8 in mass ratio by product and acetylene black and PTFE binders:1:1 uniformly mixing, the slurry mixed is applied
It is layed onto above nickel foam, is placed into the air drying cabinet that temperature setting is 80 DEG C and processing is dried.To the electrode handled well
Piece compressing tablet process, pressure are set as 15Mpa, finally carry out electrochemical property test, show that its specific capacitance is 450F/g.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (8)
1. a kind of Hydrothermal preparation method of cobaltosic oxide nano cube, which is characterized in that described method includes following steps：
1) cobalt salt, alkali, surfactant is weighed respectively to dissolve in deionized water, obtain 40~60g/L cobalt salt solutions, 55~
77g/L aqueous slkalis, 6~10g/L surfactant solutions；
2) isometric cobalt salt solution, aqueous slkali is respectively taken to carry out water bath with thermostatic control respectively, after agitating and heating is uniform, by the alkali
Solution is added in cobalt salt solution, and surfactant solution is added after the reaction was complete, obtains mixed solution；
3) mixed solution is transferred in sealed shell of tank, under air-proof condition, is mixed containing cobalt salt, alkali, surfactant to described
It closes solution and carries out hydro-thermal process, obtain black precipitate；
4) black precipitate is washed through deionized water, absolute ethyl alcohol successively, it is dry under air atmosphere, obtain four oxidation
Three cobalt nano cubics；
5) cobaltosic oxide nano cube is mixed with conductive agent and binder, slurry is obtained after being sufficiently stirred；
6) painting method is used, coating is uniformly scraped to Tu in treated nickel foam, processing is dried, is pressed later
Piece processing.
2. the Hydrothermal preparation method of cobaltosic oxide nano cube according to claim 1, which is characterized in that in step 1,
The cobalt salt is cobalt acetate, cobalt nitrate or cobaltous sulfate；The alkali is sodium hydroxide, potassium hydroxide；The surfactant is poly-
Ethylene glycol -200, neopelex, lauryl sodium sulfate.
3. the Hydrothermal preparation method of cobaltosic oxide nano cube according to claim 1, which is characterized in that in step 2,
The temperature of the water bath with thermostatic control is 45~55 DEG C, and the time is 5~10min；The volume that surfactant is added is that cobalt salt is molten
The 10~15% of liquid product；The stirring is carried out using electric mixing device, and the rotating speed of described device is 200~500 revs/min.
4. the Hydrothermal preparation method of cobaltosic oxide nano cube according to claim 1, which is characterized in that in step 3,
The temperature of the hydro-thermal process is 130~180 DEG C, and the time is 30~40 hours.
5. the Hydrothermal preparation method of cobaltosic oxide nano cube according to claim 1, which is characterized in that in step 4,
The drying temperature is 60~90 DEG C.
6. cobaltosic oxide nano cube is in preparing electrode slice made from a kind of Hydrothermal preparation method according to claim 1
Purposes, which is characterized in that the cobaltosic oxide nano cube is mixed with conductive agent and binder, is obtained after being sufficiently stirred
Slurry；The slurry is uniformly scraped into Tu in pretreated nickel foam, dry, tabletting is to get the electrode slice.
7. purposes according to claim 6, which is characterized in that the cobaltosic oxide nano cube, conductive agent and bonding
The mass ratio of agent is 8~7.5:1~1.5:1；The conductive agent is porous activated carbon or acetylene black, and the binder is PTFE
Ethanol solution.
8. purposes according to claim 6, which is characterized in that the drying temperature is 50~80 DEG C, and when tabletting presses
Power is 13~15MPa.
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| CN106348350A (en) * | 2016-10-17 | 2017-01-25 | 宿州学院 | Preparation method for nanometer cube cobaltosic oxide |
| CN107628649A (en) * | 2017-08-23 | 2018-01-26 | 国网湖南省电力公司 | Distributed power source energy storage material cobaltosic oxide nano cube and its application |
| CN108010740A (en) * | 2017-11-24 | 2018-05-08 | 北京欧美中科学技术研究院 | A kind of ultracapacitor |
| CN108172782B (en) * | 2017-12-13 | 2021-06-04 | 郑州大学 | Preparation method and application of carbon-coated porous cobaltous oxide nano material with shell-core structure |
| CN109628949B (en) * | 2019-01-31 | 2020-05-26 | 鲍君杰 | Method for preparing cobaltosic oxide by electrolytic method |
| CN112023926B (en) * | 2020-08-05 | 2022-02-18 | 兰州大学 | Electro-catalytic hydrogen evolution material and preparation method and application thereof |
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| CN103213950A (en) * | 2013-03-29 | 2013-07-24 | 北京航空航天大学 | Hydroxides and preparation method of oxide hollow structure nano material of hydroxides |
| CN104795253A (en) * | 2015-04-17 | 2015-07-22 | 天津大学 | Preparation method of hollow cobaltosic oxide microball materials and application for manufacturing electrodes |
| CN104916454A (en) * | 2015-04-17 | 2015-09-16 | 天津大学 | Preparation method for graphene like cobaltosic oxide nano film material and application of electrode slice |
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| CN103754959B (en) * | 2013-12-31 | 2016-05-04 | 常州博杰新能源材料有限公司 | A kind of preparation method of large granular spherical cobaltosic oxide |
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| CN103213950A (en) * | 2013-03-29 | 2013-07-24 | 北京航空航天大学 | Hydroxides and preparation method of oxide hollow structure nano material of hydroxides |
| CN104795253A (en) * | 2015-04-17 | 2015-07-22 | 天津大学 | Preparation method of hollow cobaltosic oxide microball materials and application for manufacturing electrodes |
| CN104916454A (en) * | 2015-04-17 | 2015-09-16 | 天津大学 | Preparation method for graphene like cobaltosic oxide nano film material and application of electrode slice |
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